• Title/Summary/Keyword: osmium analysis

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Determination of osmium using sulfurous acid as reductant by ICP-AES (Sulfurous acid 환원제를 이용한 ICP-AES에 의한 Osmium의 정량 분석)

  • Park, Han-Seok;Kim, Kang-Jin
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.251-254
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    • 2007
  • In this study, a convenient, fast and accurate inductively coupled plasma atomic emission spectrometry (ICP-AES) method has been optimized for the determination of osmium in aqueous solutions. The method makes use of the reaction of sulfurous acid with osmium to quantitative conversion of volatile Os(VIII) to non-volatile Os(IV) in the pH range 2-10. The response was found to be stabilized immediately after sulfurous acid reacted with osmium. The precision was calculated to be 0.5-4.5 % (RSD) under various ICP-AES conditions. The detection limit was 2.5-57.7 ng/g based on $3{\sigma}$ of the blank response (n=3) using a concentric flow nebulization.

Electrochemical behavior and Application of Osmium-Cupferron Complex (오스뮴-쿠페론의 전기화학적 행동 및 응용)

  • Kwon, Young-Soon;Chong, Mee-Young
    • Analytical Science and Technology
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    • v.16 no.3
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    • pp.198-205
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    • 2003
  • The ammonium salt of nitrosophenylhydroxylamine, called cupferron, has been used not only as the ligand but also as an oxidizing agent for adsorptive catalytic stripping voltammetry (AdCtSV). Cyclic voltammetry was used for elucidating the electrochemical behavior of Os-cupferron complex in 1 mM phosphate buffer. The optimal conditions for osmium analysis were found to be 1 mM phosphate buffer solution (pH 6.0) containing 0.1 mM cupferron at scan rate of 100 mV/s. By using the plot of reduction peak currents of linear scan voltammograms vs. osmium concentration, the detection limit was $1.0{\times}10^{-7}M$.

Hydrogenation of trans-Cinnamaldehyde with Hydrido-Carbonyl Osmium(II) Complexes of Chelating Phosphine Ligands

  • 정민교;허성;이원용;전무진
    • Bulletin of the Korean Chemical Society
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    • v.18 no.8
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    • pp.806-810
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    • 1997
  • A series of new hydridocarbonyl osmium(Ⅱ) complexes, OsHCl(CO)(PPh3)(L-L)[L-L=Ph2P(CH2)nPPh2 (n=1 (1), 2 (2), 3 (3), cis-Ph2PCH=CHPPh2 (4), and Fe(η5-C5H4PPh2)2 (5)] has been synthesized from OsHCl(CO)(PPh3)3 and chelating diphosphines. These complexes have been characterized by IR, 1H NMR and elemental analysis. The catalytic activities of these complexes both for the transfer hydrogenation of trans-cinnamaldehyde with 2-propanol as the hydrogen donor, and for the selective hydrogenation of trans-cinnamaldehyde with H2, have been examined. Complexes (1)-(5) were shown to have higher selectivities for the transfer hydrogenation of the C=O bond of aldehyde than for the transfer hydrogenation of the C=C bond of aldehyde. The selectivities for the transfer hydrogenation with 2-propanol as well as for the hydrogenation with H2 have been found to decrease in the order 3 > 5 > 2 > 4 > 1. Complex (3) has shown to possess almost 90% of the selectivity to cinnamyl alcohol for transfer hydrogenation. It is also found that there is a correlation between the ν(CO) of each complex and the hydrogenation, of the C=O bond of trans-cinnamaldehyde. Overall, the selectivities with the complexes (1)-(5) are greater for the transfer hydrogenation with 2-propanol than for the hydrogenation with H2.

Preparation of Cross-sectional Specimen for High Resolution Observation of Coating Structure and Visualization of Styrene/butadiene Latex Binder (고배율 도공층 구조 및 S/B latex 분포 분석을 위한 도공층 횡단면 제작)

  • Kim, Chae-Hoon;Youn, Hye-Jung;Lee, Hak-Lae
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.44 no.4
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    • pp.16-24
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    • 2012
  • To characterize the coating structure, diverse methods such as mercury intrusion, nitrogen adsorption and oil absorption methods have been developed and widely employed. These indirect techniques, however, have some limitation to explain the actual coating structure. Recently microscopic observation methods have been tried for analyzing structural characteristics of coating layers. Preparation of the undamaged cross section of a coating layer is essential for obtaining high quality image for analysis. In this study, distortion-free cross-section of the coating layer was prepared using a grinding and polishing technique. The coated paper was embedded in epoxy resin and cured. After curing the resin block it was ground with abrasive papers and then polished with diamond particle suspension and nylon cloth. Polished coating layer was sufficient enough to obtain undamaged cross sectional images with scanning electron microscope under backscattered electron image mode. In addition, the SEM images allowed distinction of the coating layer components. Also S/B latex film formed between pigment particles was visualized by osmium tetroxide staining. Pore size distribution and pore orientation were evaluated by image analysis from SEM cross-sectional images.

Distribution of the Quantum Dot Nano-particles that Penetrate Skin and Distinction of Combined Osmium Tetroxide in Electron Microscopic Analysis (피부로 침투된 양자점 나노입자의 분포와 전자현미경 분석 시 발견되는 오스뮴산 결합물과의 구분)

  • Choi, Ki-Ju;Park, Sang-Yong;Lee, Jeong-Min;Shin, Heon-Sub;Yang, Jung-Eun;Lee, Don-Gil;Mavonov, Garfurjon T.;Yi, Tae-Hoo
    • Applied Microscopy
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    • v.42 no.1
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    • pp.1-7
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    • 2012
  • The possibility of nanoparticles (NPs) in biotechnology had been discussed by biomedical investigators. Here we report to suggest a solution and problems when using electron microscopy to determine the distribution of quantum dots (QDs) nanoparticles that penetrate skin. The results of this study showed that NPs were able to penetrate stratum corneum (SC) and sebocyte via hair follicle. However, we have found artifacts such as nanoparticles that are produced from combination of free fatty acid and osmium tetroxide during specimen preparation. It is usually difficult to identify NPs. Therefore, we tried to resolve these problems by comparing the cross-correlation image pattern that are derived from the images of sample that had been processed differently. This method can contribute to more accurate interpretation and minimal errors during the analysis using quantum dot as tracer.

Composition Survey and Analysis of Non-Pt Oxygen Reduction Catalysts for Proton Exchange Membrane Fuel Cells (고체 고분자 연료전지용 비백금계 산소환원촉매 조성 조사 및 분석)

  • Kwon, Kyung-Jung
    • Journal of the Korean Electrochemical Society
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    • v.15 no.1
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    • pp.12-18
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    • 2012
  • The prohibitively high cost of Pt catalyst might be the biggest barrier for the commercialization of proton exchange membrane fuel cells (PEMFC) of which wide application is expected. Worldwide research efforts for the development of alternative to Pt oxygen reduction reaction (ORR) catalyst are made recently. One of the important considerations in the catalyst development is durability issue as well as economic aspect. From this point of view, platinum group metals (PGM) except Pt can be a candidate for replacing Pt catalyst because the material properties and the catalytic activity of PGM are expected to be similar to Pt. In contrast to Ir, Rh and Os to which not so much attention has been paid as an ORR catalyst, Pd that is most similar to Pt in terms of material properties and catalytic activity and Ru that is in the form of chalcogenide have been studied intensively. Activity comparison between non-Pt and Pt oxygen reduction catalysts by half cell test using RDE (rotating disk electrode) or PEMFC MEA (membrane electrode assembly) operation indicates that Pd-based catalysts show the most similar activity to Pt. In this paper we analyze the composition of PGM ORR catalyst in literature to promote the development of non-Pt ORR catalyst.